HRID1381220
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3.5 g. of 4-(4-chlorophenoxy)-3-pyrrolidinol, 1.8 g. of dimethylcarbamyl chloride and 1.7 g. of triethylamine in 300 ml of methylene chloride was stirred for 60 hr. The solvent was removed under vacuum, 300 ml of benezene was added and the mixture was refluxed for 2 hr., then filtered. After solvent evaporation, the residue was dissolved in cyclohexane-benzene and charcoaled. The product was then crystallized, collected by filtration and recrystallized from cyclohexane-benzene; m.p. 137°-142° C.
WORKUP
后处理
- customThe solvent was removed under vacuum, 300 ml of benezene
- additionwas added
- temperaturethe mixture was refluxed for 2 hr
- filtration, then filtered
- customAfter solvent evaporation
- dissolutionthe residue was dissolved in cyclohexane-benzene
- customThe product was then crystallized
- filtrationcollected by filtration
- customrecrystallized from cyclohexane-benzene